3种牛黄中胆汁酸类成分的含量测定与比较  

Determination and Comparison of Multiple Kinds of Bi1e Acids in Three Kinds of Calculus Bovis

作　　者：张宇静[1,2] 夏晶[2] 曹帅[2] 仇佳思 季申[2] 

机构地区：[1]中国医药工业研究总院上海医药工业研究院,上海200040 [2]上海市食品药品检验所,上海201203

出　　处：《中药新药与临床药理》2016年第4期546-551,共6页Traditional Chinese Drug Research and Clinical Pharmacology

基　　金：国家自然科学基金(81473347);上海市科学技术委员会项目(15DZ0502700);国家药典委员会人工牛黄质量标准专项研究

摘　　要：目的建立超高效液相色谱-蒸发光散射检测器(UPLC-ELSD)法同时测定天然牛黄、人工牛黄、体外培育牛黄中10种胆汁酸以及胆固醇,并比较3种牛黄中胆汁酸类成分的异同。方法采用ACQUITY UPLC HSS T3色谱柱(2.1 mm×50 mm,1.8μm),甲醇-10 mmol·L^(-1)甲酸铵(p H=3.5)为流动相,梯度洗脱,流速0.3m L·min^(-1),柱温:35℃,ELSD检测器漂移管温度65℃。结果所建立的方法可有效分离10种胆汁酸以及胆固醇,各项方法学考察均符合要求,测定结果显示3种牛黄的胆汁酸类成分在种类和含量上存在一定差异。结论本方法简便、准确、重复性好,可用于牛黄类药材中胆汁酸类成分的质量控制,并为其他胆酸类药物的测定提供参考。Objective To establish an ultra-high performance liquid chromatography-evaporative light-scattering detector（UPLC-ELSD） method for simultaneous determination and comparison of ten bile acids and cholesterol in natural,artificial and in-vitro cultured Calculus Bovis.Methods The separation was achieved on Acquity HSS T3column（2.1 mm×50 mm,1.8 μm） by gradient eluent with mobile phase consisting of methanol and 10 mmol·L^（-1） ammonium formate buffer, and the flow rate was 0.3 m L·min^（-1）.The column temperature was 35 ℃, and the temperature of the drift tube was 65 ℃. Results Ten bile acids and cholesterol were effectively separated, and investigations of methodology met the requirements.The results of determination showed that three kinds of Calculus Bovis had different kinds of bile acids, and the contents of bile acids also varied.Conclusion The established method is simple,accurate and reproducible,which can be used to control the quality of bile acids in Calculus Bovis and will supply a reference for the determination of other drugs containing bile acids.

关 键 词：牛黄 胆汁酸 含量测定 质量控制 超高效液相色谱-蒸发光散射检测器法 

分 类 号：R284.1[医药卫生—中药学]